纳米Fe_3O_4分离富集-悬浮进样-氢化物发生原子荧光法测定砷形态  

Analysis of Arsenic Speciation by Coupling Fe_3O_4 Nanoparticles Separation with Slurry Sampling and Hydride Generation Atomic Fluorescence Spectrometry

作　　者：安明日[1] 陈明丽[1] 王建华[1] 

机构地区：[1]东北大学分析科学研究中心,沈阳110819

出　　处：《分析化学》2013年第1期105-109,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21075013);中央高校基本科研业务费(Nos.N100305003,N110705002,N110805001);教育部新教师基金(No.20100042120027)资助项目

摘　　要：研究了以纳米Fe3O4为固相吸附剂对痕量无机砷形态的吸附与分离富集,建立了无需洗脱分离的悬浮进样-氢化物发生-原子荧光法测定砷形态的方法。选择的反应体系为0.64 g/L Fe3O4悬浮液-1.0%(m/V)NaBH4溶液-5.0%(V/V)HCl(pH 8),进样5.0 mL时,得到本方法的检出限为13.5 ng/L;As(Ⅲ)浓度在0.05～3.5μg/L范围内呈良好的线性关系;测定0.5μg/L As(Ⅲ)的精密度RSD=3.4%。用国家标准物质GBW10010(大米)验证了本方法测定砷的准确性,测定结果(0.101±0.010μg/g)与标准值(0.102±0.008μg/g)吻合。采用本方法测定了近海海水和雪水样品中的无机砷形态,并进行了加标回收实验。对As(Ⅲ)和As(Ⅴ)的加标回收率在95%～110%之间,结果令人满意。Fe3 04 nano-particles as adsorbent were investigated for the adsorption preconcentration of arsenic species, and a slurry sampling procedure was developed by coupling with hydride generation-atomic fluorescence spectrometry for arsenic determination and inorganic arsenic speciation. In this process, the elution procedure was eliminated which simplifies the entire operation. Under optimal conditions, e.g. , pH 8, 0.64 g/L Fe304 slurry, 1.0% （m/V） NaBH4, 5.0% （V/V） HC1, 5.0 mL sample solution, a detection limit of 13.5 ng/L was achieved for arsenic within a linear range of O. 05-3.5 μg/L, along with a precision of 3.4% RSD at 0.5 μg/L As（I）. The procedure was validated by analyzing arsenic in a certified reference material GBW 10010 （rice）, a fair agreement between the obtained value and the certified value was achieved. The speciation of inorganic arsenic in coastal sea water and snow water samples was also performed.

关 键 词：悬浮进样 纳米FE3O4 砷形态分析 氢化物发生-原子荧光光谱法 

分 类 号：O657.31[理学—分析化学]